反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
8-bromo-6-chloro-9-methyl-9H-purine (175 mg, 0.71 mmol) was combined with 4-(2-keto-1-benzimidazolinyl)piperidine (185 mg, 0.85 mmol) and dissolved in ethanol (2 mL). The resulting solution was warmed to 100° C. in a sealed tube for 15 minutes. A precipitate formed which was collected and washed with ethanol. An amount of 225 mg of a tan solid was isolated, which was 80% pure an indicated by LCMS analysis. A portion of this material was purified by prep HPLC to provide 6 mg of a white solid. 1H NMR (400 MHz, DMSO-d6): δ 10.80 (s, 1H), 8.21 (s, 1H), 7.14-7.00 (m, 1H), 6.88 (m, 3H), 5.38 (s, 2H), 4.48 (m, 1H), 3.62 (s, 3H), 3.13 (s, 2H), 2.25 (m, 2H), 1.78 (m, 2H). EI (MS) for C18H18BrN7O, found 428.
WORKUP
后处理
- customA precipitate formed which
- customwas collected
- washwashed with ethanol